CN105413720A - Silver phosphate based compound catalysis unit bonding construction method - Google Patents
Silver phosphate based compound catalysis unit bonding construction method Download PDFInfo
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- CN105413720A CN105413720A CN201510748867.XA CN201510748867A CN105413720A CN 105413720 A CN105413720 A CN 105413720A CN 201510748867 A CN201510748867 A CN 201510748867A CN 105413720 A CN105413720 A CN 105413720A
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- silver orthophosphate
- silver phosphate
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- titanium dioxide
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Abstract
The invention belongs to the technical field of material chemistry, and particularly relates to a novel silver phosphate based compound catalysis unit bonding construction method. Firstly, a liquid membrane transmission system is built, a large specific surface area silver phosphate based ordered porous structure in an ordered shape is obtained by the aid of the regulating effect of small organic molecules, a nano-scale thick anatase titanium dioxide layer is combined on the surface of the structure by the aid of molecular bonding technology, and an efficiently degraded silver phosphate/titanium dioxide heterostructure compound microsystem with a compact structure is constructed. Excellent photocatalytic activity of silver phosphate is made full use of, visible light serves as a light source, and organic pollutants on the surface of the silver phosphate based compound microsystem are rapidly degraded. A novel silver phosphate based compound catalysis unit constructed by the method is ordered in structure and high in degradation efficiency, the usage amount of silver phosphate is greatly decreased, usage cost is effectively reduced, and a novel efficient catalyst is provided for organic pollutant treatment.
Description
Technical field
The invention belongs to technical field of material chemistry, be specifically related to a kind of bonding construction method of Novel phosphoric acid money base composite catalyzing unit.
Background technology
In recent years, the environmental pollution be on the rise and energy shortage have become two large global problems, receive much concern at numerous areas.Semiconductor light-catalyst is acknowledged as and solves one of energy shortage and the promising technology of problem of environmental pollution most, the target contaminant because a kind of method it providing easy low consumption is effectively degraded, utilizes inexhaustible and free of contamination energy resources (sunshine) to carry out lasting light catalytic degradation.Low quantum yield and limited photoresponse region significantly limit the application of semiconductor light-catalyst.Silver orthophosphate (Ag
3pO
4) a large amount of photons can be caught, have high quantum yield (90%), in visible region, response range is wide.For the above-mentioned reasons, silver orthophosphate is considered to the important materials breaking semi-conducting material bottleneck.But, although Ag
3pO
4material under visible light degradating organic dye time show fabulous photo-catalysis capability, but seriously limit its practical application due to the unstability defect of self.In recent years, the selfdecomposition problem solving silver orthophosphate was devoted in a series of research, such as: by setting up heterojunction structure, as Ag
3pO
4/ AgX, Ag
3pO
4/ In (OH)
3, Ag
3pO
4/ CeO
2, Ag
3pO
4/ TiO
2, Ag
3pO
4/ Graphene, Ag
3pO
4/ Fe
3o
4, Ag
3pO
4/ SnO
2, Ag
3pO
4/ Ag, Ag
3pO
4/ carbon points etc. are to improve stability and efficiency.Because selfdecomposition phenomenon cannot thoroughly be eliminated, improve photocatalysis efficiency when reducing selfdecomposition as far as possible further and become more effective mode.And the technology of silver orthophosphate surface recombination other materials, be the key factor affecting silver orthophosphate base heterojunction structure photocatalysis effect.
In visible-light photocatalyst research, the composite photo-catalyst that Qiu Fengxian etc. are visible light-responded in patent " a kind of preparation method of visible light-responded composite photo-catalyst and application thereof " (application number: CN201510024586), it first obtains gluey silver orthophosphate by silver salt and phosphate, take multi-walled carbon nano-tubes as carrier again, prepare visible light-responded photochemical catalyst by deposition-precipitation; The catalyst prepared by the method can be used for the RhB dyestuff in degradation water solution, has simple to operate, that degradation rate is high feature.Yang Ping etc. are referred to a kind of silver/silver orthophosphate improved silica composite particles and preparation method thereof in " a kind of silver/silver orthophosphate improved silica composite particles and preparation method thereof " (application number: CN201510069024), main using silica nanometer, micron ball as host material, the sodium dihydrogen phosphate and the hydrogen peroxide that add different amount after surface functional group functionalization again stir.This method utilizes the controllable growth of silica surface silver nano-grain furthermore achieved that the growth that silver orthophosphate is controlled and the controlled adjustment with silver-colored mol ratio, method is simple, and have good photocatalysis performance, therefore there is good application prospect in fields such as environmental improvements.Yu Fei etc. have invented a kind of method of graphene-based hydrogel adsorbent of load silver orthophosphate, glutathione is added by after the ultrasonic stripping of the graphite oxide aqueous solution, and temperature control 80 DEG C keeps 12h under air-proof condition, obtain the hydrogel containing glutathione, remove residual glutathione with distilled water immersion, then in hydrogel, add AgNO
3the aqueous solution reacts, and obtains the hydrogel of loaded Ag ion; And then add NaH
2pO
4the aqueous solution reacts, and obtains the graphene-based hydrogel adsorbent of load silver orthophosphate.It improves than Graphene greatly to the adsorption capacity of methyl orange, and makes can be recycled, and recycles 3 times, and it still can reach 405.316-514.553mg/g(application number to Adsorption of Methyl Orange ability: CN201510134734).The in situ Precipitation that Ma Ni adopts in patent " silver orthophosphate/reduced graphene/titanic oxide nano compound material and preparation method " (application number: CN201510159088) has prepared silver orthophosphate/reduced graphene/titanic oxide nano compound material, wherein, reduced graphene nanometer sheet is coated on the spherical tio2 nano grain surface that size is about 300nm, the silver orthophosphate nano particle of about 10nm is adsorbed on titanium dioxide nano-particle surface, forms a kind of pine nut type structure.This catalyst is a kind of efficient, low cost, stable visible light catalyst, and preparation process is simple, easy to operate, is applicable to extensive preparation and suitability for industrialized production.Shi Weidong etc. utilize hydro-thermal method and the precipitation method, obtained visible light-responded silver orthophosphate/tungsten oxide heterojunction type photocatalytic material, it is made up of tungsten oxide and silver orthophosphate, tungsten oxide is nano-sheet, and silver orthophosphate is graininess, and silver orthophosphate nano particle homoepitaxial is on tungstic oxide nano-sheets surface, both amount of substance ratios are 1:0.3 ~ 1.8, this material is used for degradation of methylene blue dyestuff, and through degraded in 20 minutes, degradation rate can reach 97%(application number: CN201410744255).Dai Youzhi etc. provide a kind of visible-light response type core-shell structure magnetic composite photo-catalyst carbosphere zinc ferrite silver orthophosphate (CMSsZnFe
2o
4ag
3pO
4) preparations and applicatio.It for core, adopts solvent-thermal method and in situ Precipitation by zinc ferrite (ZnFe with carbosphere (CMSs)
2o
4), silver orthophosphate (Ag
3pO
4) load is surperficial at it successively, obtained two-layer core shell structure composite catalyst CMSsZnFe
2o
4ag
3pO
4.Compare pure Ag
3pO
4, it is high that composite photo-catalyst prepared by this invention has visible absorption intensity, the advantages such as Magneto separate performance is good, and anti-light corrosivity is strong.This composite photo-catalyst is applied to process 2,4-Dichlorophenol organic wastewater with difficult degradation thereby, 150 minutes to 20mg/L2,4-Dichlorophenol solution removal rate reaches 96.56%, reuse the 4th time, still can reach 86.21%(application number to 2,4-Dichlorophenol solution removal rate: CN201410648012).Yang Yefeng etc. propose and form silver orthophosphate/titanic oxide nano compound material by silver orthophosphate nano particle and titanium dioxide nanofiber with mol ratio 0.2 ~ 2:1 in patent " a kind of silver orthophosphate/titanic oxide nano compound material and preparation method thereof " (application number: CN201410629901), and the load of silver orthophosphate nano particle forms hetero-junctions on titanium dioxide nanofiber surface.Composite of the present invention all demonstrates stronger catalytic activity at ultraviolet light and visible region; And method is simple, reproducible, synthesis condition is gentle, with low cost, is easy to suitability for industrialized production.
Be not difficult to find out from existing Research foundation, silver orthophosphate based composite catalysis material has very excellent visible light catalytic efficiency, how to realize the bonding tightness between silver orthophosphate and composite better, reduce the obstruction in electronic transmission process, the stability of further raising material and catalytic performance are the technical barriers of highly research further.Given this, the present invention creatively proposes a kind of brand-new bonding construction technology and obtains phosphoric acid money base photoelectricity heterojunction structure, to improve the performance of silver orthophosphate based photocatalyst, extends its service life.The catalyst product of the method is the vesicular texture of pattern rule, compared with the existing technology, the specific area of catalysis material of the present invention is larger, catalytic activity is higher, can degradable organic pollutant effectively, be a kind of so far Novel phosphoric acid money base catalysis heterogeneous building block with how empty shape structure that there is not been reported.
Summary of the invention
The object of the invention is to the bonding construction method proposing a kind of silver orthophosphate based composite catalysis unit, acquisition catalytic performance is superior, the new catalytic unit of good stability, solves the undesirable problem of catalyst visible light photocatalytic degradation water effect of existing pure titinium dioxide or carried titanium dioxide simultaneously; The catalyst that the present invention obtains utilizes the construction unit advantage of micro-system, significantly reduces the use amount of silver orthophosphate, can catalyze and degrade organic pollutants under visible light illumination, for environmental pollution improvement provides a kind of novel effective catalyst.
The present invention proposes a kind of bonding construction method of silver orthophosphate based composite catalysis unit, and its concrete steps will complete in two steps:
The first step is the preparation of silver orthophosphate ordered structure: establish Liquid Membrane Transport system, with biological semi-permeable film in conjunction with organic active small molecular composition composite shuttering, controls the quantity of formation of nucleus and the growth rate of crystal by Liquid Membrane Transport; Utilize-the OH that composite shuttering contains ,-COOH isoreactivity group, realizes the tropism control to crystal growth; And the pore passage structure that pellicle contains, space confinement effect can be played to crystal growth.Therefore, can by changing organic molecule, the synergy between regulation and control biological semi-permeable film and space structure, thus realize the Effective Regulation of silver orthophosphate crystal morphology, structure.In silver orthophosphate ordered structure preparation process, the conditions on its such as the length in reaction time, the temperature of reaction also have very important impact.
Second step: at the nano titanium oxide of silver orthophosphate plane of crystal compound anatase titanium dioxide.The product that the first step obtains is placed in the aqueous solution of titanate ester, add ethanol to be hydrolyzed generation hydroxide, the group such as hydroxyl, carboxyl that the hydroxyl produced contains with silver orthophosphate surface is again acted on by hydrogen bond etc. and combining, thermal dehydration process again, is just compounded in the surface of silver orthophosphate crystal by titanium dioxide.Due in silver orthophosphate and titanium dioxide recombination process, mainly by means of the effect of chemical bond, hydrogen bond, therefore, it is possible to realize combining closely of titanium dioxide and silver orthophosphate.
Tool of the present invention has the following advantages:
1, construct out close structure, regular silver orthophosphate compound micro-system first, directly utilize sunshine efficient catalytic degradable organic pollutant, break away from the past catalyst to the restriction of light conditions;
2, the invention provides a kind of new photodissociation pollution administration system, Stability Analysis of Structures, convenient and efficient, life-span be long, not easily catalyst poisoning occur, its cost is not enough precious metals platinum catalyst ten thousand/.
3, the preparation method that phosphoric acid money base degradation catalyst is stablized in a kind of energy preparation is proposed first.Due to silver orthophosphate hyperactivity, can decompose when preparations and applicatio, a lot of problem is caused to production and use.The present invention is by the method at its surface bond titanium dioxide, and effectively prevent and cause moment during Synthesis and applications to be decomposed due to silver orthophosphate hyperactivity, this is that additive method cannot realize.
4, the phosphoric acid money base catalyst unit prepared by this method is porous and hierarchical structure, and channel diameter, mostly at 50 ~ 300nm, substantially increases the quantity of the active sites on surface.From microcosmic, due to small-size effect, the silver orthophosphate of nano pore is much lower for visible light reflectance compared with conventional micron level silver orthophosphate, so can energy in high efficiency absorption visible ray, it is converted into the energy required for intermolecular electron transfer, this is also make nano silver when carrying out catalytic action, the one of the main reasons that efficiency is higher than micron order.From macroscopically, this microreactor has unique multi-pore channel structure, makes it have very large specific area, has and further optimize catalytic effect.
5, the present invention can add the type of template by changing, and realizes the artificial adjustment of the particle diameter to phosphoric acid money base catalyst unit, duct size and distribution.Compare with existing method, not only product catalyst performance is good, and realizes the artificially controlled of pattern and size, meets different application demands.
6, the phosphoric acid money base catalyst unit prepared of the present invention under visible light illumination, and show extremely excellent photocatalysis performance, only a few minutes can realize the whole degradeds to organic dyestuff such as rhodamine Bs.
Detailed description of the invention
Below by specific embodiment, the present invention is further illustrated.
embodiment 1:
Measure 10mL0.5mol/LNaH
2pO
4the aqueous solution is as in conical flask, and after the sealing of egg film, be inverted in the beaker filling 10mL1.5mol/L liquor argenti nitratis ophthalmicus, ambient temperatare puts 24 hours, and centrifugation obtains silver orthophosphate product.The silver orthophosphate product of acquisition is placed in the aqueous solution of titanate ester, adds ethanol and to be hydrolyzed generation hydroxide, the group such as hydroxyl, carboxyl that the hydroxyl of generation contains with silver orthophosphate surface is again acted on by hydrogen bond etc. and combining, then 200
othe process of C thermal dehydration, is just compounded in the surface of silver orthophosphate crystal by titanium dioxide, obtain porous calcium phosphate money base composite catalyzing unit.
embodiment 2
Measure 10mL0.5mol/LNaH
2pO
4the aqueous solution is as in conical flask, after the sealing of egg film, be inverted in the beaker filling 10mL1.5mol/L liquor argenti nitratis ophthalmicus, reaction solution both sides add 1mL0.14g/L triton x-100 solution respectively, ambient temperatare puts 24 hours, and centrifugation obtains silver orthophosphate product.The silver orthophosphate product of acquisition is placed in the aqueous solution of titanate ester, adds ethanol and to be hydrolyzed generation hydroxide, the group such as hydroxyl, carboxyl that the hydroxyl of generation contains with silver orthophosphate surface is again acted on by hydrogen bond etc. and combining, then 200
othe process of C thermal dehydration, is just compounded in the surface of silver orthophosphate crystal by titanium dioxide, obtain porous calcium phosphate money base composite catalyzing unit.
embodiment 3
Measure 10mL0.5mol/LNaH
2pO
4the aqueous solution is as in conical flask, and after the sealing of egg film, be inverted in the beaker filling 10mL1.5mol/L liquor argenti nitratis ophthalmicus, reaction solution both sides add 1mL0.14g/L polyacrylamide solution respectively, and ambient temperatare puts 24 hours, and centrifugation obtains silver orthophosphate product.The silver orthophosphate product of acquisition is placed in the aqueous solution of titanate ester, adds ethanol and to be hydrolyzed generation hydroxide, the group such as hydroxyl, carboxyl that the hydroxyl of generation contains with silver orthophosphate surface is again acted on by hydrogen bond etc. and combining, then 200
othe process of C thermal dehydration, is just compounded in the surface of silver orthophosphate crystal by titanium dioxide, obtain porous calcium phosphate money base composite catalyzing unit.
embodiment 4
Measure 10mL0.5mol/LNaH
2pO
4the aqueous solution is as in conical flask, and after the sealing of egg film, be inverted in the beaker filling 10mL1.5mol/L liquor argenti nitratis ophthalmicus, reaction solution both sides add 1mL0.14g/L polyglycol solution respectively, and ambient temperatare puts 24 hours, and centrifugation obtains silver orthophosphate product.The silver orthophosphate product of acquisition is placed in the aqueous solution of titanate ester, adds ethanol and to be hydrolyzed generation hydroxide, the group such as hydroxyl, carboxyl that the hydroxyl of generation contains with silver orthophosphate surface is again acted on by hydrogen bond etc. and combining, then 200
othe process of C thermal dehydration, is just compounded in the surface of silver orthophosphate crystal by titanium dioxide, obtain porous calcium phosphate money base composite catalyzing unit.
embodiment 5
Measure 10mL0.5mol/LNaH
2pO
4the aqueous solution is as in conical flask, and after the sealing of egg film, be inverted in the beaker filling 10mL1.5mol/L liquor argenti nitratis ophthalmicus, reaction solution both sides add 1mL2.8g/L triton x-100 solution respectively, and ambient temperatare puts 24 hours, and centrifugation obtains silver orthophosphate product.The silver orthophosphate product of acquisition is placed in the aqueous solution of titanate ester, adds ethanol and to be hydrolyzed generation hydroxide, the group such as hydroxyl, carboxyl that the hydroxyl of generation contains with silver orthophosphate surface is again acted on by hydrogen bond etc. and combining, then 200
othe process of C thermal dehydration, is just compounded in the surface of silver orthophosphate crystal by titanium dioxide, obtain porous calcium phosphate money base composite catalyzing unit.
embodiment 6
Measure 10mL0.5mol/LNaH
2pO
4the aqueous solution is as in conical flask, and after the sealing of egg film, be inverted in the beaker filling 10mL1.5mol/L liquor argenti nitratis ophthalmicus, reaction solution both sides add 1mL2.8g/L polyacrylamide solution respectively, and ambient temperatare puts 24 hours, and centrifugation obtains silver orthophosphate product.The silver orthophosphate product of acquisition is placed in the aqueous solution of titanate ester, adds ethanol and to be hydrolyzed generation hydroxide, the group such as hydroxyl, carboxyl that the hydroxyl of generation contains with silver orthophosphate surface is again acted on by hydrogen bond etc. and combining, then 200
othe process of C thermal dehydration, is just compounded in the surface of silver orthophosphate crystal by titanium dioxide, obtain porous calcium phosphate money base composite catalyzing unit.
embodiment 7
Measure 10mL0.5mol/LNaH
2pO
4the aqueous solution is as in conical flask, and after the sealing of egg film, be inverted in the beaker filling 10mL1.5mol/L liquor argenti nitratis ophthalmicus, reaction solution both sides add 1mL2.8g/L triton x-100 solution respectively, and ambient temperatare puts 24 hours, and centrifugation obtains silver orthophosphate product.The silver orthophosphate product of acquisition is placed in the aqueous solution of titanate ester, adds ethanol and to be hydrolyzed generation hydroxide, the group such as hydroxyl, carboxyl that the hydroxyl of generation contains with silver orthophosphate surface is again acted on by hydrogen bond etc. and combining, then 250
othe process of C thermal dehydration, is just compounded in the surface of silver orthophosphate crystal by titanium dioxide, obtain porous calcium phosphate money base composite catalyzing unit.
embodiment 8
Measure 10mL0.5mol/LNaH
2pO
4the aqueous solution is as in conical flask, and after the sealing of egg film, be inverted in the beaker filling 10mL1.5mol/L liquor argenti nitratis ophthalmicus, reaction solution both sides add 1mL2.8g/L triton x-100 solution respectively, and ambient temperatare puts 24 hours, and centrifugation obtains silver orthophosphate product.The silver orthophosphate product of acquisition is placed in the aqueous solution of titanate ester, adds ethanol and to be hydrolyzed generation hydroxide, the group such as hydroxyl, carboxyl that the hydroxyl of generation contains with silver orthophosphate surface is again acted on by hydrogen bond etc. and combining, then 300
othe process of C thermal dehydration, is just compounded in the surface of silver orthophosphate crystal by titanium dioxide, obtain porous calcium phosphate money base composite catalyzing unit.
Claims (4)
1. the present invention proposes a kind of bonding construction method of silver orthophosphate based composite catalysis unit, its concrete preparation technology completes in two steps: the first step is the preparation of silver orthophosphate ordered structure, set up Liquid Membrane Transport system, with pellicle in conjunction with organic active small molecular composition composite shuttering, control the quantity of formation of nucleus and the growth rate of crystal by Liquid Membrane Transport; Utilize-the OH that composite shuttering contains ,-COOH isoreactivity group, realizes the tropism control to crystal growth; And the pore passage structure that pellicle contains, space confinement effect can be played to crystal growth, thus obtain different-shape, there is the silver orthophosphate sill of different ducts size and distribution; Second step is nano level anatase titanium dioxide at silver orthophosphate plane of crystal composite thickness, silver orthophosphate sill by first step acquisition is placed in the aqueous solution of tetrabutyl titanate, add ethanol to be hydrolyzed generation hydroxide, the group such as hydroxyl, carboxyl that the hydroxyl produced contains with silver orthophosphate surface is again combined by bonding actions such as hydrogen bonds, thermal dehydration process again, titanium dioxide is bonded in the surface of silver orthophosphate crystal, obtains novel porous calcium phosphate money base composite catalyzing unit.
2., according to claims 1, the pellicle used is egg film, and small molecule organic compound is triton x-100, polyacrylamide, acrylamide, polyethylene glycol.
3. according to claim 1, it is characterized in that the thermal dehydration treatment temperature in second step is 200 ~ 300 degrees Celsius.
4., according to claims 1, it is characterized in that silver orthophosphate based composite catalysis unit is the silver orthophosphate/titanium dioxide heterogeneous structure of porous.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108323529A (en) * | 2018-04-10 | 2018-07-27 | 上海泽铭环境科技有限公司 | A kind of nanometer compound fungicide used in environmental area |
| CN109012708A (en) * | 2018-07-17 | 2018-12-18 | 江苏大学 | A kind of fold-type titania fiber load nano silver composite material and preparation method |
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| CN102274738A (en) * | 2011-06-16 | 2011-12-14 | 华东理工大学 | Complex nanocatalyst which is easy to recycle and preparation method thereof |
| CN102657228A (en) * | 2012-05-21 | 2012-09-12 | 华东理工大学 | Method for in-situ preparing nano-silver compound bactericide |
| CN104258886A (en) * | 2014-09-16 | 2015-01-07 | 上海电力学院 | Silver phosphate/oxygen vacancy type titanium dioxide compound photocatalyst and preparation method thereof |
| CN104909428A (en) * | 2015-05-14 | 2015-09-16 | 南京大学 | Device and method for treating hard-to-degrade organic waste water by combined treatment of Ag3PO4/TiO2 catalyst and low-temperature plasma |
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2015
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102274738A (en) * | 2011-06-16 | 2011-12-14 | 华东理工大学 | Complex nanocatalyst which is easy to recycle and preparation method thereof |
| CN102657228A (en) * | 2012-05-21 | 2012-09-12 | 华东理工大学 | Method for in-situ preparing nano-silver compound bactericide |
| CN104258886A (en) * | 2014-09-16 | 2015-01-07 | 上海电力学院 | Silver phosphate/oxygen vacancy type titanium dioxide compound photocatalyst and preparation method thereof |
| CN104909428A (en) * | 2015-05-14 | 2015-09-16 | 南京大学 | Device and method for treating hard-to-degrade organic waste water by combined treatment of Ag3PO4/TiO2 catalyst and low-temperature plasma |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108323529A (en) * | 2018-04-10 | 2018-07-27 | 上海泽铭环境科技有限公司 | A kind of nanometer compound fungicide used in environmental area |
| CN109012708A (en) * | 2018-07-17 | 2018-12-18 | 江苏大学 | A kind of fold-type titania fiber load nano silver composite material and preparation method |
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